CN110108827B - Method for simultaneously determining eight active ingredients in antipyretic and antitoxic tablet - Google Patents

Method for simultaneously determining eight active ingredients in antipyretic and antitoxic tablet Download PDF

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CN110108827B
CN110108827B CN201910444207.0A CN201910444207A CN110108827B CN 110108827 B CN110108827 B CN 110108827B CN 201910444207 A CN201910444207 A CN 201910444207A CN 110108827 B CN110108827 B CN 110108827B
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acetonitrile
antitoxic
antipyretic
tablet
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CN110108827A (en
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孙艳涛
苏斌
赵磊
赵国升
刘春玲
邵嘉乐
杨志超
李美锡
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Jilin Normal University
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Abstract

The invention discloses a method for simultaneously determining eight active ingredients in a antipyretic and antitoxic tablet, which comprises the following steps: (1) preparing a reference substance solution; (2) test solutionPreparing a liquid; (3) separation and detection: the chromatographic column is Agilent TC-C18(ii) a The mobile phase composition is acetonitrile 0.2 percent of phosphoric acid, and the gradient elution condition is that 13 percent to 14 percent of acetonitrile is 0 to 14min, 14 percent to 22 percent of acetonitrile is 14 to 15min, 22 percent to 22 percent of acetonitrile is 15 to 20min, 22 percent to 25 percent of acetonitrile is 20 to 25min, 25 percent to 35 percent of acetonitrile is 25 to 30min, 35 percent to 43 percent of acetonitrile is 30 to 38min, 43 percent to 53 percent of acetonitrile is 38 to 40min, 53 percent to 53 percent of acetonitrile is 40 to 45min, and 53 percent to 83 percent of acetonitrile is 45 to 50 min; the detection wavelength is 0-15min 303nm, 15-20min 230nm, 20-50min 280 nm; the flow rate was 1.0 mL/min‑1(ii) a The column temperature is 30 ℃; the amount of sample was 10. mu.L. The method has the advantages of good chromatographic peak separation, strong specificity, accuracy, reliability, simplicity and convenience, and provides a theoretical basis for quality control of antipyretic and antitoxic tablets.

Description

Method for simultaneously determining eight active ingredients in antipyretic and antitoxic tablet
Technical Field
The invention belongs to the technical field of medicines, and relates to a method for detecting active ingredients in a Chinese patent medicine antipyretic and antitoxic tablet, in particular to a method for simultaneously determining eight active ingredients in the antipyretic and antitoxic tablet.
Background
The Chinese patent medicine is used as an important component of the medical treasury in China and has an irreplaceable effect in the process of promoting the development of the medical industry in China. Because the active ingredients of the Chinese patent medicine are complex, the effective substance basis of the medicine is not clear, and the single medicinal material is easily influenced by factors such as variety, producing area, processing method and the like, the quality evaluation of the Chinese patent medicine becomes an obstacle which hinders the Chinese patent medicine from moving to modernization and internationalization. With the development of modern analysis and test means, the quality control of Chinese patent medicines can qualitatively and quantitatively analyze the main chemical components of a certain medicine by using high performance liquid chromatography, and breaks through the single quality control of the Chinese patent medicines by means of microscopic identification and TLC analysis in the past, however, most of the methods are limited to the quantification of single chemical components, and at least one chemical component is still selected to quantitatively analyze the Chinese medicinal materials or the Chinese patent medicines under most of the existing 2015 edition of Chinese pharmacopoeia. The Chinese patent medicine is used as a complete preparation, and emphasizes the synergistic effect of the medicinal materials, so that the quality of the Chinese patent medicine is difficult to control really by using a single effective component or index component. Therefore, modern separation technology is required to realize comprehensive qualitative and quantitative analysis of multiple effective components in Chinese patent medicine, so as to reveal the diversity and controllability of the effective components of Chinese patent medicine, develop from single index to multiple detection indexes, improve the means of quality control of Chinese patent medicine, and promote the Chinese patent medicine to further move to internationalization.
The antipyretic and antitoxic tablet is a light yellow sugar-coated tablet, is brownish, slightly fragrant in smell, sweet in taste and bitter after sugar coating is removed, and is mainly used for epidemic cold, fever, cold intolerance, anhidrosis and headache, thirst and dry throat, aching pain of limbs and mumps and gall. Thin-layer identification of radix Puerariae, radix Paeoniae Rubra, and radix Angelicae Dahuricae and content determination of baicalin are added in the quality standards of the second volume of the drug Standard of the ministry of health (Chinese medicinal component preparation) and the first part of the Chinese pharmacopoeia of 2010 edition. Because the antipyretic and antitoxic tablet contains more than ten components such as trichosanthes root, kudzuvine root, baical skullcap root, red paeony root, dahurian angelica root and the like, the existing quality standard is not strong in specificity, and the quality of the medicine cannot be comprehensively evaluated. Research papers have determined that single components in antipyretic and antitoxic tablets, such as puerarin, paeoniflorin, imperatorin and harpagoside, and reports of simultaneous determination of multiple components are not found. Therefore, a method for rapidly, accurately and comprehensively separating and detecting multiple active ingredients of the antipyretic and antitoxic tablet is needed to be established so as to better perform quality monitoring and medication safety on the product.
Disclosure of Invention
The invention aims to provide a method for simultaneously determining eight active ingredients in a antipyretic and antitoxic tablet, which can simultaneously determine the contents of puerarin, paeoniflorin, liquiritin, 5-O-methyl visammol glycoside, baicalin, arctiin, phillyrin and arctigenin in the antipyretic and antitoxic tablet, has the advantages of simple method, stability and good reproducibility, and can be used for quality control of the medicine.
In order to realize the purpose, the invention is realized by adopting the following technical scheme:
a method for simultaneously determining eight active ingredients in a antipyretic and antitoxic tablet comprises the following specific steps:
(1) preparation of control solutions: accurately weighing control substances including puerarin, penoniflorin, liquiritin, 5-O-methyl visammol glycoside, baicalin, phillyrin, arctiin and arctigenin, respectively, placing in a 5mL volumetric flask, adding methanol to desired volume, shaking to obtain constant volume, and controlling the concentration to be 0.404 mg/mL-1、0.35mg·mL-1、0.609mg·mL-1、0.376mg·mL-1、0.388mg·mL-1、0.29mg·mL-1、0.594mg·mL-1And 0.464 mg. mL-1(ii) a Respectively precisely sucking 50 mu L of eight single reference substance stock solutions, placing the eight single reference substance stock solutions into the same 5mL volumetric flask, and adding methanol to a constant volume to obtain a mixed reference substance solution;
(2) preparation of a test solution: taking a sample of the antipyretic and antitoxic tablet, removing sugar coating to show brown color, grinding in a mortar uniformly, weighing accurately, placing in a 10mL volumetric flask, adding 75% methanol by volume percent for dissolving, shaking uniformly at constant volume, and performing ultrasonic treatment for 30min to obtain a concentration of 12.124 mg/mL-1；
(3) Separation and detection: respectively injecting the mixed reference substance solution and the test substance solution into an Agilent 1100 liquid chromatograph, and detecting by adopting the following chromatographic conditions: the chromatographic column is Agilent TC-C18(ii) a VWD detector: switching a detection wavelength, wherein the detection wavelength is a switching wavelength condition as follows:
TABLE 1 detection wavelength
Figure GDA0002101478230000021
The mobile phase composition is acetonitrile and 0.2 percent phosphoric acid, and the mobile phase is subjected to the following gradient elution conditions:
TABLE 2 flow phase ratio example
Figure GDA0002101478230000022
Flow rate 1.0 mL/min-1(ii) a Column temperature: 30 ℃; sample introduction amount: and 10 mu L of the extract is obtained.
The invention has the following advantages and positive effects:
1. the method adopts High Performance Liquid Chromatography (HPLC) to realize the simultaneous separation and determination of the content of 8 effective components in the antipyretic and antitoxic tablet by using gradient elution and wavelength switching under the same experimental condition, has simple operation and good precision, accuracy, reproducibility and stability, and can provide theoretical basis and scientific basis for the comprehensive evaluation and control of the quality of the antipyretic and antitoxic tablet.
2. The chromatography established by the invention can better separate and determine the content of puerarin, paeoniflorin, liquiritin, 5-O-methyl visammioside, baicalin, arctiin, phillyrin and arctigenin in the antipyretic and antitoxic tablet, the peak shape of the chromatographic peak is good, the separation degree is higher, the concentration of 8 components and the peak area show good linear relation under the chromatographic condition, and the recovery rate of each component is better.
Drawings
FIG. 1 chromatogram of a mixed standard solution of the invention.
FIG. 2 is a chromatogram of a test solution of the present invention.
FIG. 3 is a chromatogram of puerarin of the present invention.
FIG. 4 chromatogram of paeoniflorin of the present invention.
FIG. 5 chromatogram of liquiritin of the present invention.
FIG. 6 chromatogram of 5-O-methylvisammioside according to the invention.
FIG. 7 chromatogram of baicalin in the present invention.
FIG. 8 chromatogram of arctiin of the present invention.
FIG. 9 chromatogram of phillyrin of the present invention.
FIG. 10 is a chromatogram of arctigenin according to the present invention.
FIG. 11 is a standard curve of puerarin of the present invention.
FIG. 12 is a standard curve of paeoniflorin of the present invention.
FIG. 13 is a standard curve of liquiritin of the present invention.
FIG. 14 is a standard curve of 5-O-methylvisammioside according to the invention.
FIG. 15 is a standard curve of baicalin in the present invention.
FIG. 16 is a standard curve of arctiin according to the present invention.
FIG. 17 is a standard curve of phillyrin of the present invention.
FIG. 18 is a standard curve of arctigenin according to the present invention.
Detailed Description
The invention is further described below in conjunction with the appended drawings and detailed description so that those skilled in the art may better understand the invention, but the invention is not limited thereto.
Instrument and reagent
The instrument comprises the following steps: agilent 1100 hplc, usa; shimadzu ultraviolet spectrophotometer UV 2550; GWA-UN4 series ultrapure water purifier (Beijing general analysis instruments, LLC); FA1104N ten thousandth analytical balance (manufactured by balance instruments factory, shanghai precision scientific instruments ltd); SK5200H ultrasonic cleaner (200W59Hz Shanghai Kegan instruments Co., Ltd.).
Reagent testing: the antipyretic and antitoxic tablet is purchased from Tongrentang, Beijing, with the batch number of Z11021172; the puerarin reference substance is purchased from China food and drug research institute with the batch number of 110752-; the paeoniflorin reference substance is purchased from China food and drug research institute with the batch number of 110736-201337; the liquiritin reference substance is purchased from the institute of Chinese food and drug, with the batch number of 111610-; the 5-0-methylvisammioside reference substance is purchased from China food and drug research institute with the batch number of 111523-201208; the baicalin reference substance is purchased from the institute of Chinese food and drug, with the batch number of 110715-one 201619; the forsythin reference substance is purchased from China institute of food and drug, with the batch number of 110821-; the arctiin reference substance is purchased from China food and drug research institute with the batch number of 110819-; arctigenin is purchased from Shanghai Hotan Biotechnology corporation, lot number 7770-78-7; acetonitrile (TEDIA, chromatographically pure), phosphoric acid (national pharmaceutical group chemical agents ltd, analytical pure), and water as ultrapure water.
Example 1
A method for simultaneously determining eight active ingredients in a antipyretic and antitoxic tablet comprises the following specific steps:
(1) preparation of control solutions: accurately weighing control substances including 2.02mg of puerarin, 1.75mg of paeoniflorin, 3.045mg of liquiritin, 1.88mg of 5-O-methylvisammol glycoside, 1.94mg of baicalin, 1.45mg of forsythin, 2.97mg of arctiin and 2.32mg of arctigenin in a 5mL volumetric flask, adding methanol to a constant volume, and shaking to obtain a constant volume with a concentration of 0.404 mg/mL-1、0.35mg·mL-1、0.609mg·mL-1、0.376mg·mL-1、0.388mg·mL-1、0.29mg·mL-1、0.594mg·mL-1And 0.464 mg. mL-1(ii) a Precisely sucking 50 mu L of eight single reference substance stock solutions respectively, placing the eight single reference substance stock solutions into the same 5mL volumetric flask, and adding methanol to a constant volume to obtain a mixed reference substance solution;
(2) preparation of a test solution: taking a sample of the antipyretic and antitoxic tablet, removing sugar coating to show brown color, putting into a mortar for grinding uniformly, accurately weighing 0.12124g, putting into a 10mL volumetric flask, adding 75% methanol by volume for dissolving, shaking uniformly at constant volume, and performing ultrasonic treatment for 30min to obtain a concentration of 12.124 mg/mL-1；
(3) Separation detection
The final chromatographic conditions were determined as: a chromatographic column: TC-C18(4.6 mm. times.250 mm, 5 μm); VWD detector: the mobile phase composition is acetonitrile 0.2 percent of phosphoric acid, and the gradient elution condition is that 13 percent to 14 percent of acetonitrile is 0 to 14min, 14 percent to 22 percent of acetonitrile is 14 to 15min, 22 percent to 22 percent of acetonitrile is 15 to 20min, 22 percent to 25 percent of acetonitrile is 20 to 25min, 25 percent to 35 percent of acetonitrile is 25 to 30min, 35 percent to 43 percent of acetonitrile is 30 to 38min, 43 percent to 53 percent of acetonitrile is 38 to 40min, 53 percent to 53 percent of acetonitrile is 40 to 45min, and 53 percent to 83 percent of acetonitrile is 45 to 50 min; the detection wavelength is 0-15min 303nm, 15-20min 230nm and 20-50min 280 nm; the flow rate was 1.0 mL/min-1(ii) a The column temperature is 30 ℃; the sample injection amount is 10 mu L;
under the chromatographic condition, the retention time of puerarin, paeoniflorin, liquiritin, 5-O-methyl visammioside, baicalin, phillyrin, arctiin and arctigenin is 11.854min, 18.676min, 21.879min, 24.128min, 31.887min, 32.523min, 33.103min and 42.355min respectively, and corresponding chromatographic peaks are observed in a chromatogram of a test sample, as shown in fig. 1 to fig. 10.
Comparative example 1
In the invention, when the gradient elution condition is determined, methanol-water solution is adopted for gradient elution to separate the component to be detected, and the specific gradient elution condition is as follows: 0-5min 5% -5% methanol, 5-10min 5% -30% methanol, 10-25min 30% -30% methanol, 25-45min 30% -60% methanol, 45-55min 60% -80% methanol, 55-70min 80% -80% methanol, but the substances are not separated well at the moment;
comparative example 2
In the invention, when the gradient elution condition is determined, acetonitrile-water solution is adopted for gradient elution to separate the component to be detected, and the specific gradient elution condition is as follows: 0-10min 15% -15% acetonitrile, 10-12min 15% -28% acetonitrile, 12-17min 28% -28% acetonitrile, 17-27min 28% -55% acetonitrile, 27-42min 55% -85% acetonitrile, 42-52min 85% -85% acetonitrile, but the phenomenon that the chromatographic peak of partial substances has tailing is still found at the time;
through multiple selection of gradient elution conditions, the invention finally discovers that when acetonitrile is subjected to gradient elution, wherein the acetonitrile comprises 0.2% of phosphoric acid, 0-14min 13% -14% of acetonitrile, 14-15min 14% -22% of acetonitrile, 15-20min 22% -22% of acetonitrile, 20-25min 22% -25% of acetonitrile, 25-30min 25% -35% of acetonitrile, 30-38min 35% -43% of acetonitrile, 38-40min 43% -53% of acetonitrile, 40-45min 53% -53% of acetonitrile and 45-50min 53% -83% of acetonitrile, chromatographic peaks can be well separated, the peak shape is good, the analysis time can be effectively shortened, and the analysis requirements are met.
Comparative example 3
Selection of detection wavelength: carrying out ultraviolet spectrum scanning on puerarin, paeoniflorin, liquiritin, 5-O-methylvisammol glycoside, baicalin, phillyrin, arctiin and arctigenin according to the literature, and determining the maximum ultraviolet absorption wavelengths of the puerarin, the paeoniflorin, the liquiritin, the 5-O-methylvisammol glycoside, the baicalin, the phillyrin, the arctiin and the arctigenin to be 303nm, 230nm, 276nm, 254nm, 280nm, 277nm and 280nm respectively, so that the detection is carried out by adopting the switching wavelength at the corresponding peak-off time of 0-15min 303nm, 15-20min 230nm and 20-50; the initial detection wavelength of 280nm is selected in the experiment, but the quantitative analysis of the experiment is influenced to a certain extent due to the small peak areas of puerarin and paeoniflorin under the wavelength, so that a wavelength switching method is adopted.
Methodology examination
The linear relationship is: precisely sucking 0.2, 1, 5, 10, 15 and 20 μ L of single reference substance solution, respectively, injecting into a liquid chromatograph, measuring the sample according to the above chromatographic conditions, and taking the peak area as ordinate, the concentration as abscissa, and the peak area as linear regression equation to the mass. The linear relationships are shown in FIGS. 11-18, and the regression equation results for each component are shown in Table 3.
TABLE 3 Linear relation equation
Figure GDA0002101478230000051
And (3) precision experiment: and precisely sucking the mixed reference substance solution, carrying out continuous sample injection for 6 times, measuring the peak area of the mixed reference substance solution, and calculating RSD (reference signal density) with the result shown in Table 4, wherein the experimental result shows that the precision of the instrument is good.
TABLE 4 precision test
Figure GDA0002101478230000052
And (3) stability test: the same sample solution was injected at 0, 2, 4, 6, 8, 10 and 12 hours according to the above chromatographic conditions, and the stability was determined, the results are shown in Table 5, and the experimental data show that the sample solution is substantially stable within 12 hours.
TABLE 5 stability test
Figure GDA0002101478230000061
And (3) repeatability test: 5 parts of the same batch of test sample are taken, the solution is prepared according to the preparation method of the test sample solution, and the result is shown in the table 6 according to the measurement of the chromatographic conditions, which indicates that the method has good repeatability.
TABLE 6 weightsRenaturation experiments (units mg g)-1)
Figure GDA0002101478230000062
Determination of content
Calculated by peak area data, the contents of puerarin, penoniflorin, liquiritin, 5-O-methyl visammol glycoside, baicalin, phillyrin, arctiin and arctigenin are respectively 6.43mg g-1、0.78mg·g-1、0.2326mg·g-1、0.168mg·g-1、8.09mg·g-1、0.25mg·g-1、5.87mg·g-1And 0.67mg g-1。
Recovery test
And (3) carrying out a recovery rate experiment according to the content measurement result, precisely weighing 5 parts of the test sample with known content, respectively adding a certain amount of puerarin, paeoniflorin, liquiritin, 5-O-methylvisammioside, baicalin, phillyrin, arctiin and arctigenin reference substances, operating according to the test sample preparation and measurement method, calculating the standard recovery rate, and obtaining the result shown in table 7.
TABLE 7 sample recovery test results
Figure GDA0002101478230000063
Figure GDA0002101478230000071
In conclusion, the high performance liquid chromatography established by the invention is used for simultaneously measuring the content in the antipyretic and antitoxic tablet, has the characteristics of simple and convenient operation, good precision and high repeatability, and can comprehensively and effectively control the quality of the antipyretic and antitoxic tablet.

Claims (1)

1. A method for simultaneously determining eight active ingredients in a antipyretic and antitoxic tablet is characterized by comprising the following specific steps:
(1) preparation of control solutions: accurately weighing control substances including puerarin, penoniflorin, liquiritin, 5-O-methyl visammol glycoside, baicalin, phillyrin, arctiin and arctigenin, respectively, placing in a 5mL volumetric flask, adding methanol to desired volume, shaking to obtain constant volume, and controlling the concentration to be 0.404 mg/mL-1、0.35mg·mL-1、0.609mg·mL-1、0.376mg·mL-1、0.388mg·mL-1、0.29mg·mL-1、0.594mg·mL-1And 0.464 mg. mL-1(ii) a Respectively precisely sucking 50 mu L of eight single reference substance stock solutions, placing the eight single reference substance stock solutions into the same 5mL volumetric flask, and adding methanol to a constant volume to obtain a mixed reference substance solution;
(2) preparation of a test solution: taking a sample of the antipyretic and antitoxic tablet, removing sugar coating to show brown color, grinding in a mortar uniformly, weighing accurately, placing in a 10mL volumetric flask, adding 75% methanol by volume percent for dissolving, shaking uniformly at constant volume, and performing ultrasonic treatment for 30min to obtain a concentration of 12.124 mg/mL-1；
(3) Separation and detection: respectively injecting the mixed reference substance solution and the test substance solution into an Agilent 1100 liquid chromatograph, and detecting by adopting the following chromatographic conditions: the chromatographic column is Agilent TC-C18(ii) a VWD detector: switching a detection wavelength, wherein the detection wavelength is a switching wavelength condition as follows:
TABLE 1 detection wavelength
Figure FDA0003033046380000011
The mobile phase composition is acetonitrile and 0.2 percent phosphoric acid, and the mobile phase is subjected to the following gradient elution conditions:
TABLE 2 flow phase ratio example
Figure FDA0003033046380000012
Flow rate 1.0 mL/min-1(ii) a Column temperature: 30 ℃; sample introduction amount: and 10 mu L of the extract is obtained.
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